CA1066174A - Method for producing compound thin films - Google Patents
Method for producing compound thin filmsInfo
- Publication number
- CA1066174A CA1066174A CA240,388A CA240388A CA1066174A CA 1066174 A CA1066174 A CA 1066174A CA 240388 A CA240388 A CA 240388A CA 1066174 A CA1066174 A CA 1066174A
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- atoms
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
- C23C16/45548—Atomic layer deposition [ALD] characterized by the apparatus having arrangements for gas injection at different locations of the reactor for each ALD half-reaction
- C23C16/45551—Atomic layer deposition [ALD] characterized by the apparatus having arrangements for gas injection at different locations of the reactor for each ALD half-reaction for relative movement of the substrate and the gas injectors or half-reaction reactor compartments
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02422—Non-crystalline insulating materials, e.g. glass, polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/02543—Phosphides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02557—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S148/00—Metal treatment
- Y10S148/025—Deposition multi-step
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S148/00—Metal treatment
- Y10S148/072—Heterojunctions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S148/00—Metal treatment
- Y10S148/169—Vacuum deposition, e.g. including molecular beam epitaxy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S438/00—Semiconductor device manufacturing: process
- Y10S438/935—Gas flow control
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S438/00—Semiconductor device manufacturing: process
- Y10S438/971—Stoichiometric control of host substrate composition
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- Condensed Matter Physics & Semiconductors (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
- Physical Vapour Deposition (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE:
A method of growing compound thin films of single atomic layers by sequential surface reaction steps between the single elements of the compound and a body surface. The method of the invention comprises subjecting in each reaction step the body surface to interaction with atoms of a single element in vapour phase at a partial pressure sufficiently high and over a period of time sufficiently long to cause collisions on the surface of the single element atoms in excess of the number of atoms in one single atomic layer of the surface, and maintaining the surface at a temperature sufficiently high for the surface reaction to occur and too high for the reacting vapour to condense itself on the surface. The invention enables one to form a single atomic layer by a means which is self-determining and which does not permit the formation of layers of greater thickness.
A method of growing compound thin films of single atomic layers by sequential surface reaction steps between the single elements of the compound and a body surface. The method of the invention comprises subjecting in each reaction step the body surface to interaction with atoms of a single element in vapour phase at a partial pressure sufficiently high and over a period of time sufficiently long to cause collisions on the surface of the single element atoms in excess of the number of atoms in one single atomic layer of the surface, and maintaining the surface at a temperature sufficiently high for the surface reaction to occur and too high for the reacting vapour to condense itself on the surface. The invention enables one to form a single atomic layer by a means which is self-determining and which does not permit the formation of layers of greater thickness.
Description
The present invention concerns a method for producing compound thin films of single atomic layers by sequential surface reaction steps between the single elements of the compound and a body surface.
Among the methods for producing compound thin films from the gaseous phase, the most important method is vacuum evaporation. This is effected either directly using the particular compound as the source of the vapors or by simultaneous evaporation of the different chemical element components from different sources and thus subjecting the substrate on which the compound thin film is to be formed simultaneously to the-vapors of the elements. In other words, the substrate is simultaneously subjected to the vapors from the evaporation of the compound or from the simultaneous evaporation of the elements forming the compound.
In the first case, the major drawback resides in the decomposition of the compound into its components which makes it extremely difficult, if not impossible, to control the stoichiometry of the film that is produced, the stoichiometry generally tending to change during the course of the evaporation process.
When the gases for the formation of the thin film are supplied by simultaneous evaporation of the component elements from which the compound is formed, good stoichiometry requires extremely close control of the evaporation rates of the different compounds, or selective back evaporation of the more readily evaporating component. As in the case of evaporation from the compound itself, the nucleation properties and crystal structure of the film are inadequately controllable in the case of subjecting the substrate to the vapors from simultaneous evaporation of the components thereof.
` 1066174 When a single crystal substrate is used in the manner known in the art, the selective back evaporation can be made sufficiently efficient so that the growing film continues the crystal structure of the substrate. This type of procedure is known as Molecular seam Epitaxy and is described in J. Vac.
Sci. Technol., Vol. 10, No. 5, Sept./Oct. 1973, L.L. Chang et al.
"Structures Grown by Molecular Beam Epitaxy".
When the completed compound is used as a source, the decomposition of the compound can be reduced in manner known in the art by means of sputtering techniques wherein the material to be transposed is detached from the source by ion bombardment. The best stoichiometry is usually attained in sputtering techniques by means of so-called bias sputtering, which is comparable to the use of back evaporation.
Generally speaking, in accordance with the invention highly oriented compound thin films are produced with almost perfect stoichiometry by alternately subjecting the substrate, one at a time, to the vapor of each of the elements of which the compound is formed.
It is accordingly a primary object of the present invention to provide a method of producing compound thin films which results in the formation of a highly oriented compound and which does this while avoiding the disadvantages of the prior art.
It is another object of the invention to provide for the production of compound thin films by the building up of single atomic layers of the elements of which the compound is formed.
In accordancewith the present invention, there is provided a method of growing compound thin films of single atomic layers by sequential surface reaction steps between the single elements of the compound and a body surface, which comprises subjecting in each reaction step the body surface C
to interaction with atoms of a single element in vapor phase at a partial pressure sufficiently high and over a period of time sufficiently long to cause collisions on the surface of the single element atoms in excess of the number of atoms in one single atomic layer of the surface, and maintaining the surface at a temperature sufficiently high for the surface reaction to occur and too high for the reacting vapor to condense itself on the surface.
The above method can be carried out with the aid of an apparatus which mainly comprises vacuum chamber means for providing an evacuated atmosphere, a pair of means including support means for supporting the body surface and a source means for forming sources for vapors of the single elements, respectively, and operating means operatively connected with one of the pair of means for operating the one means with respect to the other of the pair of means for providing sequentially on the body surface single atomic layers of the elements.
For facility of discussion, the method of the invention will often hereinafter be referred to as "atomic layer epitaxy", and will be abbreviated as "ALE".
The most important groups of compound films are the II-VI and III-V binary compounds and combinations thereof.
This is mainly due to the semiconductor characteristics of these compounds. In order to achieve successful semiconductor uses of the compounds,the crystalline structure of the films is of primary importance. For most applications this requirement is sufficiently high to restrict the useful material to single crystals only which can be made by epitaxy on a single crystal substrate. The epitaxy of compound materials is relatively difficult, compared to the epitaxy of elementary materials such as silicon and germanium. This is mainly due to the higher complexity of the compound growth, which in the case of ~' "J - 3 -~066~74 binary compounds and vapor phase epitaxy involves the existence of both the vapor and solid phases of the compound and both component elements. To obtain a good stoichiometry, one must therefore have precise control of the arrival rates or partial pressures of the component elements as well as the temperature of the substrate.
For many applications it is desirable to have the semiconductor material in thin film form on a substrate which is not a single crystal, but combines the features of low price and possibility to extensive areas. Such applications where II-VI and III-V compounds are of high interest are, for instance, solar cells, several optoelectronic devices, imaging devices, display devices, etc. Extensive use of such devices has however been limited by the poor quality of the semiconductor material obtained by deposition techniques of prior art.
Every known deposition technique in the prior art used to obtain film deposition on non-single crystal substrates includes the unavoidable feature of formation of nuclei at the beginning of the film growth. The film does not gain a continuous structure until the single microcrystals (growing nuclei) touch each other. This generally occurs when the mean thickness of the film is of the order of 100~. The resulting films have a polycrystalline (or in certain circumstances amorphous) structure. The electrical characteristics of the films are greatly affected by the polycrystalline structure of the material. Not only the electrical characteristics of the films suffer from the poor structure of the materials, but also the chemical stability, which is a necessary condition for the technical use of the films. Moreover, both the electrical and chemical characteristics of the compound films are strongly affected by deviations from stoichiometry, which deviations are most difficult to avoid in the deposition process.
~ s indicated above, the compound film generation method according to the invention is mainly characterized in that the solid-phase surface (substrate) is reacted stepwise with vapors, one at a time, each consisting only of one of the elementary component of the compound, so that as a result of surface reaction there is bound on the surface not more than one atomic layer of the element in question in each of the reaction steps.
The method of this invention provides the important advantage of epitaxy even when an amorphous substrate is used, resulting in a nucleation-free compound film which is highly oriented in the direction of film growth. An essential difference from other deposition methods resides in the fact that the film growth proceeds stepwise, atomic plane by atomic plane, resulting from a surface reaction between one component element in gas phase and the other as surface atoms in the growing compound film.
The process of the invention can be made self-balancing by maintaining the temperature of the growing surface high enough to prevent condensation of the element in each individual reaction step. Thus, for a binary film AB, where A represents an element of groups I, II, III and IV, -~
and B an element of groups VII, VI and V, the reaction is cyclically repeated, i.e., gas A reacts with a B surface forming an A surface with A-B compound bonding, then the surface is subjected to gas B, where asa result of the reaction between gas B and the A surface s-A bonding is formed resulting in a B surface, which again is subjected to A gas, etc.
When a glass substrate is used, the condition for initiation of the stepwise process is that one of the components of the compound must have sufficient bonding strength with oxygen atoms which form the surface of glass. This condition is directly fulfilled for most II-VI and III-V compounds and it ~1~
~ - 5 -"- 1066174 can, in practice, be fulfilled for all compounds suitable for ALE growth using intermediate atomic layers. If the ALE
method of the present invention is used for epitaxy on single crystals, the lattice dlrection of the substrate must fulfill the condition of component atom planes in rotation.
For a fuller understanding of the invention reference is made to the following description taken in connection with the accompanying drawings, in which:
FIG. 1 is a schematic partly sectional view of an apparatus for carrying out the method of the invention;
FIG. 2 is a transverse section of the structure of FIG. 1 taken along line II-II of FIG. 1 in the direction of the arrows;
FIG. 3 is a partly sectional schematic elevation of another embodiment of a structure for carrying out the method of the invention;
- FIG. 4 is a transverse section of the structure of FIG. 3 taken along line IV-IV of FIG. 3 in the direction of the arrows; and FIGS. 5-7 respectively illustrate schematically and partly in section three different further embodiments of structures for carrying out the method of the invention.
The apparatus of FIG. 5 provides for the reaction chamber being tightly sealed against vacuum yet permits axial movement of the structure holder. The embodiment of FIG. 6 provides for the substrate being stationary, and FIG. 7 shows a modification of the embodiment of FIG. 6 and according to which the film growth takes place on both sides of the substrate and the reaction chamber can be evacuated between each reaction step by means of a special valve means.
In the process of the invention, atomic layers are deposited of, for example element A and B, wherein element A
C generally belongs to one of the groups I, II, III or IV of the ~066174 periodic system and element B belongs to one of the groups VII, VI or V, respectively of the periodic system. The most typical films produced by the method of the invention are I-VII, II-VI or III-V compounds or oxides. According to the invention element A in gaseous phase reacts with the surface on which the film is to be grown, the surface atoms of which belong to group B, forming a single atomic layer due to the powerful B-A bond produced on the surface. All of the A atoms impinging on the surface, in addition to those which form the B-A bond immediately return to the gaseous phase in the case where the A-A bond is not sufficiently strong to prevent the back evaporation of the element A which occurs as a result of the temperature which is above the evaporation temperature of element A. When in interaction with the gaseous phase of the element A, the film that is being grown can only grow by a single atomic layer even if the number of atoms impinging on the surface considerably exceeds that which corresponds to the single or monoatomic layer.
After the surface to be grown has been in interaction with the gaseous phase of element A, it is next brought into interaction with the gaseous phase of element B. The A
atoms on the surface layer of the film now enter into the formation of a strong B-A bond by the action of the B atoms directly thereon, and the surface thus becomes covered with a single atomic layer of element B. Again, the B-B bond is unable to prevent the element B from returning to the gaseous phase because it is not sufficiently strong to do so. These alternate reaction steps are repeated until the required thickness of the A-B compound is obtained.
Some advantageous devices for carrying out the method of the invention will now be described in detail with reference to Figs. 1-7.
1066~74 Figs. 1 and 2 illustrate a vacuum apparatus confined by the chamber 10, wherein the substrates 14, on which a film is being grown, have been mounted on a disk 12 rotatable with the aid of a shaft 11. Below the disk 12 vapour sources 13a and 13b have been placed, which are mutually isolated sectors and each of which has been arranged to have a desired vapour pressure of the elementary components of the film that shall be grown. When the disk 12 is rotated the substrates 14 are alternatingly placed in interaction with the vapours of elements A (13a) and B (13b), whereby the growth of the film takes place according to the procedure of the invention, provided that the gas pressures and temperature of the substrate 14 required by the process have been furnished.
In the embodiment example of FIGS. 3 and 4 the disk 12 of the preceding example has been replaced by a ring 12b rotatable with the aid of the shaft 11 and on the outer circum-ference of which the substrates 14 have been mounted. The vapour ; - 8 -t``~ 6~74 sour~es 'iS.e, 1'j1~ arld 1~c have been placed radially around the ring 12b. Th~ speed of rotation of the ring 12a is most ~ppropriately 'bet~icen 1 and 20 r.p.sec.
An apparatus of the kind sho~m in Figs. 1 to 4, whe~ein a relati~re motion has been prov~ded between the substrates 14 and the vapour sources 13, may also be accor,1plished in that the substr~tes 14 are stationary and the vapour sources are moving.
The apparatus may also be designed so that, for instance, the substrates 14 are affixed to a member resembling a conveyor belt and which carries the substrates past the vapour sources.
It is eve~n othe~ise understood that the relative motion of sunstrates and vapour sources with reference to each other ma.y -be accomplished by a great number of different devices.
The apparatus according to Fig 5 comprises a vacuum chamber 10 .md separate reaction chambers 19a and 19b, wherc the sunstrates 14 can be moved in rotation, and vacuum-tightly sealed ill each reaction. This arrangeMent allows better isolation o the reaction steps and smaller leakage of the reaction gases, but it is mechanically more compli'cated. Improved isolation of '' the reaction steps rnay also be obtained with fe~er mechanically moving parts, using the embodiment of Figs. 6 and 7. Further according to ~ig. 5, the shaft 10a may also be moved in axial direction. A means for carrying out both movements is illustrated schematically by the block 24. A block 2~ represents schematical-ly the Tnotion control in question, and a block 22 similarly represen-ts the control of the valves 15a and 15b. The sources of the diflerent gases are indicated by reference numerals 20a and 20b. Reference numeral 21 refers to the sealing means in connection with the reaction chamb'ers 19a'and 19b.
In the apparatus shown in Fig. 6 the substrate has been mounted to be stationary on .~ base 12c, and it is kept at a suitablc tcmpera-ture with the aid of a heating member 17. The , ~06~7~
apparatus eO'.lpriS'-`S two vapour sources l3a and 13b, which are alternating,; arranged to act on the substrate 14 l'hi..s is accomplished with the aid of valves 15a and 15b fitted in pipes 16a a~d 16b, these valves opening/closin~ in alternation so that while onc o t.he valves 15a/15b is open the other valve 15b/15a is closed. The means effecting thi.s mode of operation have been schemakically represented by the block 18 and the switch k.
According to ~ig. 7 there are outside the reaction chamber 19, the sources of different gases, 20a and 20b. The substrates 14 in the chamber 10 are held in their position by special holding mcans 29 and 30.
The reaction chamber 10 is filled with the element gases in rotation~ uslng the valves 15a and 15b and they are evacuated between consecutive steps using the valve 26. In this ærran~ement the walls of the reaction chamber ~0 wlll be covered with the compound simult~leously with the growth on the su-ostrates 14, which will be covered pn both sides. A block 28 shows the means for actuating the valve 26, and the block 25 represents ltS control means.
The theoretical background of the present inve~ion is in the following described in greater detail with reference to ~he different embodiments of the invention disclosed pre-viously.
In the source thb element A is in equilibrium between its solid phase and its vapour pressure p~ at te~perature Ta (or if Ta exceeds melting point of A, equilibrium prevails between the li.quid and gaseous phases). The corresponding situation for element ~ obtains in the source 13b. In the case of a self-balancing A~ procedure the subs-trate temperature To is kept higher than the source temperatures TA and TB~ which mearls that the A and B vapours do not condense on thc substrate.
I(~ .
6G~74 In case the .~ ~t;OUlS forln a so.lid CO.~pOUlld ~i.th. oxygen, ~^rith bindi.ng ener~y high erlou~h to prevent decomposi-tion, the sub trate will be covered by a monatomi.c layer of A atoms with A-0 bonds. ~he coverage of the surface with ~ atoms can be described by the equation (assurni.ng dP~ = ~ (1 - PA) . dtj - ~A ~A0 . tA~
10PA = 1 - e Ns (1) where Ph = relative surface area covered with A atom.s X:
~A - collision density of A atoms with the surface, which has the form (accoroing to kinetic gas theury) V 2 mi~ ~ rtorr~ ~ .
NS = density of sur~ace atoms ~s~ 115 1/c~2 tAo = interaction time of the surface.with 0-atom and reacting 20gas A ~s~ .
~A0 = surface-reaction probability, of atom A wi.th O.ato~ surface, corresponding to the "sticking coefficient" in conventionai deposition methods.
The surface reaction probability d~ is a complex func-tion of the ter~perature of.the reaction surface and the pressure of t~e reacting gas. It varies widely with different ele~ents and compounds formed. For monatoMic gases ~ has been found to be higher than for biato~ic or multiatomic gases.
- From equation (~) it can be found that the relative ~0 coverage of the surface with ~ atoms approaches unity a~,ymptoti-cally ~ith increasing time of interaction.
A si~1ificant benefit of the ~ rowth is that the : 1066174 vapour pres;~re o~ ~he forn~ing compo~md has its minimum just in thc growth dl eclion, t11e strongest possible bonds occuring perpendiculclr to the surface.
If the B atoms form a solid compound with oxygen with high binding energy, the substra-te in interaction ~ith the B
sou~ce will be covered with ~ atom~ exactly as dcscribed for the interaction between it and the A aJ~oms and the glass surface.
For ~ type elements this ls not generally the case, which means that the surface of the substrate glass will remain unchanged during its interaction with B vapour.
In-the next reaction step the substrates covered witl - a monatomic layer of A atoms are placed in interaction ~ithL
the source of B atoms in gas phase. lhe surface will be covered with B atoms according to equation (1), again forming a monatomic layer of B atoms with h-B compound bond. ~he conditions valid for the vapour pressures of said monatomic B l~yer with A-B
~ - bonds and B atoms on this layer, ~Tith B-~ bonds, differ by many orders of magnitude, resulting in an extremely selective bacl-evaporation of the B atoms lacking compound bonds.
By repeated reaction steps in rotation, the surface of the substrates will be covered by a layer structure ie 0-A-~-A-B-A-B-A-B... where the first 0 stands for the surface aton iayer of the substrate and the following A-B layers form a highly oriented film sf compound AB. In the case of perfect coverage in each reaction step the total thickness of the-film is determined by the number of rotations and the lattice constant of the compound.
Using several sources with diferent elements A1...An, B1...Bm~ layer structures containing compound combina-S0 tions, such as superlat;tices, heterojunctions, etc.,may begro~m.
~ hc conditions for A~E growth, as described, may be ` J "- - 1066~74 ~efined by the terms of equation ~ or a full coverage as described abJ~e the connitions ~A0/UA t~o~ Ns ~A~ ~A tAB~ Ns and - t2) ~ ~A~UB t~ Ns must be provided.
In caaes with PA and PB directly in interaction with the reacting surface, as in ~igs. 1, 2, 3, 4, 5 and 7, the source temperatures TA and T~ are linked with ~A and ~B by equations.
~A ~ f(PA) = f(T~) ~B ~ f(P~) - f(T~) (3) ~ o ensure perfect back evaporation of the elernents having no compound bond9 ~/hich is mandatory in a self-balancing A~E process, the substrate temperature To must be sufficiently - -. far above t~e temperatures TA and T~. The upper limit of ~'0 is in principle determined by the vapour pressure of the compound.
In practice, ho~ever, when a glass substrate is used, the upper lim.it of To is generally determined by the softening point of the substrate glass. It should be noted that the lattice direction of the growing surface in A~E growth most efficiently minimizes the vapour pressure of the compound. This has been established e.g. in connection with CdSe growth, which has been carried out at To ~ 500C without any detectable back evaporation of the compound.
It is obvious that A~E growth is obtainable with several types of growing equiprnent. The essential features are the sovrce and substrate ternperatures, and step~ise interactions bet~een the substrate and the elernent vapours of the compound in rotation. ~specially ~he II-VI compound group offers great freedoln in ecluipment design, due to the high vapour pressure i066174 ~ .
oX II ~nd ~TI elerne~ts. Two principal arrangements dif-ferent fxom that de.i;cribed in ~'ig. 5 are presented in Figs. 6 and 7.
In AIE growth the interaction with a component vapou~
may be o~tained by using a gaseous compound of the element ~'nich decomposcs on the reacting surface, in analogy with the practice of chemical vapour deposition. This kind o~ reaction ma~ be accomplished e.g. with H2S, instead of S2. ~he corresponding ~urface reactions in the case of ZnS growth are X2S(g) + Zn(s) --~ ZnS(s) + H2(g) in the case of H2S, corresponding to the reaction - S2(g) + 2 Zn(s) > ZnS(s) for pure S2 gas. According to the AIæ principle the r~actions-are only possible as long as free Zn(s) surface atoms are available, ~he A~E procedure can be performed with the aid of sputter-type deposition of the component elements. In this .
case there is an inert gas or plasma present in the reaction ~ steps.
~ hen applying equation (1) to surfaces which are not per~ectly covered with the atoms causing surface reaction with the gas atoms in question~ the equation shall only be applied to the active portion of the surface. It an AB compound is grown using partial surface coverage in each or one of the process steps, the equation (1) may be modified to read ~A ~ AB
* N tab PA - PB ~ e s (4) for A-atom reaction steps and UB BA
~s tBA
P~ PA - e - (5) for B atom reaction steps, where PB and PA represent the relative coverages of B and ~ atoms on the surface before the A and B
reaction steps, respectively.
I~r ~` ~066'17~
The p~rtial coverage oi one component clement is of special irnp~ ce w]lein 7rowing cornpound films with low va~our pressure elemen-i~s o with compounds which contain different amounts of the c~mponent elements. An important exarnple of the first-mentioned is the growth of III-V compounds on a substrate which cannot be heated temperature To h:igh enough to ensure perfect back evaporation of the group III elernents. In such a case the surface reaction between group V surface atoins and and group III gaseous atoms is limited -to cause only partial coverage of group III atoms to ensure the absence of super-numerary group III atoms on the surface. ~he group V gas reaction with the surface partially covered with g~oup III
atoms can be made perfect enough to ensure the oriented nuclea-tion-free A~E growth of the compound.
Another ~mportant case in which partial surface reac-tion æteps have to be used is the growth of dioxides of elements which also have stable or relatively stable monoxi2es. The growth of tin dioxide b~ A~E technique is an illustrative example. In order to form SnO2, instead of SnO, the interaction of Sn vapour with the O surface is restricted to cause Sn coverage of a fe~ per cent only. ~he 2 interaction, effected by me~ls f 2 plasma, ensures the maximuTn nurnber of oxygen atoms to be bonded with Sn atoms, thus causing the dioxide -growth. A strong indication for use of A~E growth in such instances, too, has emerged from the observation t'nat the SnO2 layer on a glass plate shows electrical conductivity in the plane of the surface starting frorn 10 A SnO2 thic]~ness. The conductlvity shows no tumlelling effects, which is proof that the film has a continuous . crystal structure. Such films are physically extremely firm and che.nically resistant, which is in fact true for all compound filrns made by A~E techni~ues, no mattcr w}lether witn perIcc-t or partial covera~e of -the reactin~ surfacc in the individual 7~
~eaction st~p~
E~
_a~ le 1 Al,E growth for ZnS has been carried out with an equipment of ~i~s. 1 and 2 with following values of system parameter3:
- Speed of rotati.on 2 r/s - substrate material: Corning Glass 7059 - substrate temperature 320C, -the total bombardme-nt of Zn-atoms during one interaction bet~/een the surface and .
Zn vapou.r about 5 x 1015 atoms/cm2, which was measured with a quar~.crystal rate monitor, corresponding to an effective Zn vapour pressure of about 10 3 torr and equiLibri~m ~: .
temperature of about 290C for the Zn source - equilibrium temperature of the S source 100C, corresponding to a vapour pressure.of about 10 2 torr and total bombardment of S2 molecules of about 5 x 1016 molecules/cm2.
~ or a ten minutes pr~cess the film thickness was about 0.27 ~m5 for processes of 20 and ~0 minutes the thich~nesses were about 0.54 ~m and 0.80 ~ respectively.
The film structure was examined by etching techniques.
Example 2 -- A~ growth of SnO2 layers on Corning Glass 7059 substrates has been carried out using thc equipment of ~igs. 1 and.2 as follows:
- The substrate temperature ~00C
- The total amount of Sn atoms during one interaction with Sn source about 0.6 1014 atoms/cm2 .. - oxygen source is of plasma type with 10-100 mTorr total pressu.re and 40mA plas.ma cur~ent. The total bombardment of . 30 02 ions being ~ 7 1014 ions/cm2 during the interaction with the plasma source Ib " ` ~ 7~
- with speed rot:ation 1 r/s this proccss ~ives a ~rowth o~ S;~02 ~, O
film to 6~)0A in 25 minutes giVillg 0. 4.~ average growth rate during each ro1ation ~xam~le 3 A~E growth of GaP-layers on CGrning Glass 7059 substrates has been carried out using the equipment of ~i~s.
~ and 2 as follows:
- the ~ubstrate tem-perature~V300C
- the total a~nount of Ga atoms during the interacti.on with ~a source~ 1015 atoms/cm2 - the total amount of P molecules (most probably P4) bornbarding the surface during the interaction with Phosphorus oven is about 5 ' 1015 atoms/cm~
- a 0.25 p film was gro~m with these parar/1eters of substrate and sources in 25 minutes with rotation speed 1 r/s. Average growth rate was 1.7A during each cycle.
Exan~le 4 A~E grow-th of ZnS has been carried out using the equip-men-t of Fig. 7 with follo~ing system parameters: -- substrate c.g. 7059 - substrate temperature~470C
- temperature of Zn-sourcer~ 390C
- temperature of S-source~120C
- interactlon time of the Zn-source 6 sec-onds - escape time of the Zn-vapour 2 seconds - interaction time of the S-source 2 seconds - escape time of the S2-vapour 6 seconds - ~he growth occured at maximum speed within the accuracy of thiclmess measu~ent thus corresponding full coverage at each reaction step. With a 140 min process the film thickness was O,1 2 ~lm.
~x~perl~ncnts wi-th the self--balanclng ~E growth have .
~i7 . ........... ~k -f ~ 7 4 establis.~d ~ f~ct, th~t the trlo~oretical ro~rth speed ca~not be exeeded bu-t apnro~ched ..sympcoticall~J with increased time (or pres~ure) of interact;ion at each reacti.on step.
Selective e-tcning of the ZnS films made by A~E techniques has been performed Wi ch the ai~ o.t a e-tchan-t con tainin~ 60 parts H3P04, 5 parts I~03 and one part H~ at room temperature. ~he etching speed was from 10 ~m/s to 150 ~/s in the direction of the surface for 0.1 to 0.'7 ~m thick %nS films whilst no etchin~
effec t could be ~etected in the direction perpendicularly to the surface plane. ~ching of A~-SnO2 fi.lms has been possible only by electrochemical methods~
1~
Among the methods for producing compound thin films from the gaseous phase, the most important method is vacuum evaporation. This is effected either directly using the particular compound as the source of the vapors or by simultaneous evaporation of the different chemical element components from different sources and thus subjecting the substrate on which the compound thin film is to be formed simultaneously to the-vapors of the elements. In other words, the substrate is simultaneously subjected to the vapors from the evaporation of the compound or from the simultaneous evaporation of the elements forming the compound.
In the first case, the major drawback resides in the decomposition of the compound into its components which makes it extremely difficult, if not impossible, to control the stoichiometry of the film that is produced, the stoichiometry generally tending to change during the course of the evaporation process.
When the gases for the formation of the thin film are supplied by simultaneous evaporation of the component elements from which the compound is formed, good stoichiometry requires extremely close control of the evaporation rates of the different compounds, or selective back evaporation of the more readily evaporating component. As in the case of evaporation from the compound itself, the nucleation properties and crystal structure of the film are inadequately controllable in the case of subjecting the substrate to the vapors from simultaneous evaporation of the components thereof.
` 1066174 When a single crystal substrate is used in the manner known in the art, the selective back evaporation can be made sufficiently efficient so that the growing film continues the crystal structure of the substrate. This type of procedure is known as Molecular seam Epitaxy and is described in J. Vac.
Sci. Technol., Vol. 10, No. 5, Sept./Oct. 1973, L.L. Chang et al.
"Structures Grown by Molecular Beam Epitaxy".
When the completed compound is used as a source, the decomposition of the compound can be reduced in manner known in the art by means of sputtering techniques wherein the material to be transposed is detached from the source by ion bombardment. The best stoichiometry is usually attained in sputtering techniques by means of so-called bias sputtering, which is comparable to the use of back evaporation.
Generally speaking, in accordance with the invention highly oriented compound thin films are produced with almost perfect stoichiometry by alternately subjecting the substrate, one at a time, to the vapor of each of the elements of which the compound is formed.
It is accordingly a primary object of the present invention to provide a method of producing compound thin films which results in the formation of a highly oriented compound and which does this while avoiding the disadvantages of the prior art.
It is another object of the invention to provide for the production of compound thin films by the building up of single atomic layers of the elements of which the compound is formed.
In accordancewith the present invention, there is provided a method of growing compound thin films of single atomic layers by sequential surface reaction steps between the single elements of the compound and a body surface, which comprises subjecting in each reaction step the body surface C
to interaction with atoms of a single element in vapor phase at a partial pressure sufficiently high and over a period of time sufficiently long to cause collisions on the surface of the single element atoms in excess of the number of atoms in one single atomic layer of the surface, and maintaining the surface at a temperature sufficiently high for the surface reaction to occur and too high for the reacting vapor to condense itself on the surface.
The above method can be carried out with the aid of an apparatus which mainly comprises vacuum chamber means for providing an evacuated atmosphere, a pair of means including support means for supporting the body surface and a source means for forming sources for vapors of the single elements, respectively, and operating means operatively connected with one of the pair of means for operating the one means with respect to the other of the pair of means for providing sequentially on the body surface single atomic layers of the elements.
For facility of discussion, the method of the invention will often hereinafter be referred to as "atomic layer epitaxy", and will be abbreviated as "ALE".
The most important groups of compound films are the II-VI and III-V binary compounds and combinations thereof.
This is mainly due to the semiconductor characteristics of these compounds. In order to achieve successful semiconductor uses of the compounds,the crystalline structure of the films is of primary importance. For most applications this requirement is sufficiently high to restrict the useful material to single crystals only which can be made by epitaxy on a single crystal substrate. The epitaxy of compound materials is relatively difficult, compared to the epitaxy of elementary materials such as silicon and germanium. This is mainly due to the higher complexity of the compound growth, which in the case of ~' "J - 3 -~066~74 binary compounds and vapor phase epitaxy involves the existence of both the vapor and solid phases of the compound and both component elements. To obtain a good stoichiometry, one must therefore have precise control of the arrival rates or partial pressures of the component elements as well as the temperature of the substrate.
For many applications it is desirable to have the semiconductor material in thin film form on a substrate which is not a single crystal, but combines the features of low price and possibility to extensive areas. Such applications where II-VI and III-V compounds are of high interest are, for instance, solar cells, several optoelectronic devices, imaging devices, display devices, etc. Extensive use of such devices has however been limited by the poor quality of the semiconductor material obtained by deposition techniques of prior art.
Every known deposition technique in the prior art used to obtain film deposition on non-single crystal substrates includes the unavoidable feature of formation of nuclei at the beginning of the film growth. The film does not gain a continuous structure until the single microcrystals (growing nuclei) touch each other. This generally occurs when the mean thickness of the film is of the order of 100~. The resulting films have a polycrystalline (or in certain circumstances amorphous) structure. The electrical characteristics of the films are greatly affected by the polycrystalline structure of the material. Not only the electrical characteristics of the films suffer from the poor structure of the materials, but also the chemical stability, which is a necessary condition for the technical use of the films. Moreover, both the electrical and chemical characteristics of the compound films are strongly affected by deviations from stoichiometry, which deviations are most difficult to avoid in the deposition process.
~ s indicated above, the compound film generation method according to the invention is mainly characterized in that the solid-phase surface (substrate) is reacted stepwise with vapors, one at a time, each consisting only of one of the elementary component of the compound, so that as a result of surface reaction there is bound on the surface not more than one atomic layer of the element in question in each of the reaction steps.
The method of this invention provides the important advantage of epitaxy even when an amorphous substrate is used, resulting in a nucleation-free compound film which is highly oriented in the direction of film growth. An essential difference from other deposition methods resides in the fact that the film growth proceeds stepwise, atomic plane by atomic plane, resulting from a surface reaction between one component element in gas phase and the other as surface atoms in the growing compound film.
The process of the invention can be made self-balancing by maintaining the temperature of the growing surface high enough to prevent condensation of the element in each individual reaction step. Thus, for a binary film AB, where A represents an element of groups I, II, III and IV, -~
and B an element of groups VII, VI and V, the reaction is cyclically repeated, i.e., gas A reacts with a B surface forming an A surface with A-B compound bonding, then the surface is subjected to gas B, where asa result of the reaction between gas B and the A surface s-A bonding is formed resulting in a B surface, which again is subjected to A gas, etc.
When a glass substrate is used, the condition for initiation of the stepwise process is that one of the components of the compound must have sufficient bonding strength with oxygen atoms which form the surface of glass. This condition is directly fulfilled for most II-VI and III-V compounds and it ~1~
~ - 5 -"- 1066174 can, in practice, be fulfilled for all compounds suitable for ALE growth using intermediate atomic layers. If the ALE
method of the present invention is used for epitaxy on single crystals, the lattice dlrection of the substrate must fulfill the condition of component atom planes in rotation.
For a fuller understanding of the invention reference is made to the following description taken in connection with the accompanying drawings, in which:
FIG. 1 is a schematic partly sectional view of an apparatus for carrying out the method of the invention;
FIG. 2 is a transverse section of the structure of FIG. 1 taken along line II-II of FIG. 1 in the direction of the arrows;
FIG. 3 is a partly sectional schematic elevation of another embodiment of a structure for carrying out the method of the invention;
- FIG. 4 is a transverse section of the structure of FIG. 3 taken along line IV-IV of FIG. 3 in the direction of the arrows; and FIGS. 5-7 respectively illustrate schematically and partly in section three different further embodiments of structures for carrying out the method of the invention.
The apparatus of FIG. 5 provides for the reaction chamber being tightly sealed against vacuum yet permits axial movement of the structure holder. The embodiment of FIG. 6 provides for the substrate being stationary, and FIG. 7 shows a modification of the embodiment of FIG. 6 and according to which the film growth takes place on both sides of the substrate and the reaction chamber can be evacuated between each reaction step by means of a special valve means.
In the process of the invention, atomic layers are deposited of, for example element A and B, wherein element A
C generally belongs to one of the groups I, II, III or IV of the ~066174 periodic system and element B belongs to one of the groups VII, VI or V, respectively of the periodic system. The most typical films produced by the method of the invention are I-VII, II-VI or III-V compounds or oxides. According to the invention element A in gaseous phase reacts with the surface on which the film is to be grown, the surface atoms of which belong to group B, forming a single atomic layer due to the powerful B-A bond produced on the surface. All of the A atoms impinging on the surface, in addition to those which form the B-A bond immediately return to the gaseous phase in the case where the A-A bond is not sufficiently strong to prevent the back evaporation of the element A which occurs as a result of the temperature which is above the evaporation temperature of element A. When in interaction with the gaseous phase of the element A, the film that is being grown can only grow by a single atomic layer even if the number of atoms impinging on the surface considerably exceeds that which corresponds to the single or monoatomic layer.
After the surface to be grown has been in interaction with the gaseous phase of element A, it is next brought into interaction with the gaseous phase of element B. The A
atoms on the surface layer of the film now enter into the formation of a strong B-A bond by the action of the B atoms directly thereon, and the surface thus becomes covered with a single atomic layer of element B. Again, the B-B bond is unable to prevent the element B from returning to the gaseous phase because it is not sufficiently strong to do so. These alternate reaction steps are repeated until the required thickness of the A-B compound is obtained.
Some advantageous devices for carrying out the method of the invention will now be described in detail with reference to Figs. 1-7.
1066~74 Figs. 1 and 2 illustrate a vacuum apparatus confined by the chamber 10, wherein the substrates 14, on which a film is being grown, have been mounted on a disk 12 rotatable with the aid of a shaft 11. Below the disk 12 vapour sources 13a and 13b have been placed, which are mutually isolated sectors and each of which has been arranged to have a desired vapour pressure of the elementary components of the film that shall be grown. When the disk 12 is rotated the substrates 14 are alternatingly placed in interaction with the vapours of elements A (13a) and B (13b), whereby the growth of the film takes place according to the procedure of the invention, provided that the gas pressures and temperature of the substrate 14 required by the process have been furnished.
In the embodiment example of FIGS. 3 and 4 the disk 12 of the preceding example has been replaced by a ring 12b rotatable with the aid of the shaft 11 and on the outer circum-ference of which the substrates 14 have been mounted. The vapour ; - 8 -t``~ 6~74 sour~es 'iS.e, 1'j1~ arld 1~c have been placed radially around the ring 12b. Th~ speed of rotation of the ring 12a is most ~ppropriately 'bet~icen 1 and 20 r.p.sec.
An apparatus of the kind sho~m in Figs. 1 to 4, whe~ein a relati~re motion has been prov~ded between the substrates 14 and the vapour sources 13, may also be accor,1plished in that the substr~tes 14 are stationary and the vapour sources are moving.
The apparatus may also be designed so that, for instance, the substrates 14 are affixed to a member resembling a conveyor belt and which carries the substrates past the vapour sources.
It is eve~n othe~ise understood that the relative motion of sunstrates and vapour sources with reference to each other ma.y -be accomplished by a great number of different devices.
The apparatus according to Fig 5 comprises a vacuum chamber 10 .md separate reaction chambers 19a and 19b, wherc the sunstrates 14 can be moved in rotation, and vacuum-tightly sealed ill each reaction. This arrangeMent allows better isolation o the reaction steps and smaller leakage of the reaction gases, but it is mechanically more compli'cated. Improved isolation of '' the reaction steps rnay also be obtained with fe~er mechanically moving parts, using the embodiment of Figs. 6 and 7. Further according to ~ig. 5, the shaft 10a may also be moved in axial direction. A means for carrying out both movements is illustrated schematically by the block 24. A block 2~ represents schematical-ly the Tnotion control in question, and a block 22 similarly represen-ts the control of the valves 15a and 15b. The sources of the diflerent gases are indicated by reference numerals 20a and 20b. Reference numeral 21 refers to the sealing means in connection with the reaction chamb'ers 19a'and 19b.
In the apparatus shown in Fig. 6 the substrate has been mounted to be stationary on .~ base 12c, and it is kept at a suitablc tcmpera-ture with the aid of a heating member 17. The , ~06~7~
apparatus eO'.lpriS'-`S two vapour sources l3a and 13b, which are alternating,; arranged to act on the substrate 14 l'hi..s is accomplished with the aid of valves 15a and 15b fitted in pipes 16a a~d 16b, these valves opening/closin~ in alternation so that while onc o t.he valves 15a/15b is open the other valve 15b/15a is closed. The means effecting thi.s mode of operation have been schemakically represented by the block 18 and the switch k.
According to ~ig. 7 there are outside the reaction chamber 19, the sources of different gases, 20a and 20b. The substrates 14 in the chamber 10 are held in their position by special holding mcans 29 and 30.
The reaction chamber 10 is filled with the element gases in rotation~ uslng the valves 15a and 15b and they are evacuated between consecutive steps using the valve 26. In this ærran~ement the walls of the reaction chamber ~0 wlll be covered with the compound simult~leously with the growth on the su-ostrates 14, which will be covered pn both sides. A block 28 shows the means for actuating the valve 26, and the block 25 represents ltS control means.
The theoretical background of the present inve~ion is in the following described in greater detail with reference to ~he different embodiments of the invention disclosed pre-viously.
In the source thb element A is in equilibrium between its solid phase and its vapour pressure p~ at te~perature Ta (or if Ta exceeds melting point of A, equilibrium prevails between the li.quid and gaseous phases). The corresponding situation for element ~ obtains in the source 13b. In the case of a self-balancing A~ procedure the subs-trate temperature To is kept higher than the source temperatures TA and TB~ which mearls that the A and B vapours do not condense on thc substrate.
I(~ .
6G~74 In case the .~ ~t;OUlS forln a so.lid CO.~pOUlld ~i.th. oxygen, ~^rith bindi.ng ener~y high erlou~h to prevent decomposi-tion, the sub trate will be covered by a monatomi.c layer of A atoms with A-0 bonds. ~he coverage of the surface with ~ atoms can be described by the equation (assurni.ng dP~ = ~ (1 - PA) . dtj - ~A ~A0 . tA~
10PA = 1 - e Ns (1) where Ph = relative surface area covered with A atom.s X:
~A - collision density of A atoms with the surface, which has the form (accoroing to kinetic gas theury) V 2 mi~ ~ rtorr~ ~ .
NS = density of sur~ace atoms ~s~ 115 1/c~2 tAo = interaction time of the surface.with 0-atom and reacting 20gas A ~s~ .
~A0 = surface-reaction probability, of atom A wi.th O.ato~ surface, corresponding to the "sticking coefficient" in conventionai deposition methods.
The surface reaction probability d~ is a complex func-tion of the ter~perature of.the reaction surface and the pressure of t~e reacting gas. It varies widely with different ele~ents and compounds formed. For monatoMic gases ~ has been found to be higher than for biato~ic or multiatomic gases.
- From equation (~) it can be found that the relative ~0 coverage of the surface with ~ atoms approaches unity a~,ymptoti-cally ~ith increasing time of interaction.
A si~1ificant benefit of the ~ rowth is that the : 1066174 vapour pres;~re o~ ~he forn~ing compo~md has its minimum just in thc growth dl eclion, t11e strongest possible bonds occuring perpendiculclr to the surface.
If the B atoms form a solid compound with oxygen with high binding energy, the substra-te in interaction ~ith the B
sou~ce will be covered with ~ atom~ exactly as dcscribed for the interaction between it and the A aJ~oms and the glass surface.
For ~ type elements this ls not generally the case, which means that the surface of the substrate glass will remain unchanged during its interaction with B vapour.
In-the next reaction step the substrates covered witl - a monatomic layer of A atoms are placed in interaction ~ithL
the source of B atoms in gas phase. lhe surface will be covered with B atoms according to equation (1), again forming a monatomic layer of B atoms with h-B compound bond. ~he conditions valid for the vapour pressures of said monatomic B l~yer with A-B
~ - bonds and B atoms on this layer, ~Tith B-~ bonds, differ by many orders of magnitude, resulting in an extremely selective bacl-evaporation of the B atoms lacking compound bonds.
By repeated reaction steps in rotation, the surface of the substrates will be covered by a layer structure ie 0-A-~-A-B-A-B-A-B... where the first 0 stands for the surface aton iayer of the substrate and the following A-B layers form a highly oriented film sf compound AB. In the case of perfect coverage in each reaction step the total thickness of the-film is determined by the number of rotations and the lattice constant of the compound.
Using several sources with diferent elements A1...An, B1...Bm~ layer structures containing compound combina-S0 tions, such as superlat;tices, heterojunctions, etc.,may begro~m.
~ hc conditions for A~E growth, as described, may be ` J "- - 1066~74 ~efined by the terms of equation ~ or a full coverage as described abJ~e the connitions ~A0/UA t~o~ Ns ~A~ ~A tAB~ Ns and - t2) ~ ~A~UB t~ Ns must be provided.
In caaes with PA and PB directly in interaction with the reacting surface, as in ~igs. 1, 2, 3, 4, 5 and 7, the source temperatures TA and T~ are linked with ~A and ~B by equations.
~A ~ f(PA) = f(T~) ~B ~ f(P~) - f(T~) (3) ~ o ensure perfect back evaporation of the elernents having no compound bond9 ~/hich is mandatory in a self-balancing A~E process, the substrate temperature To must be sufficiently - -. far above t~e temperatures TA and T~. The upper limit of ~'0 is in principle determined by the vapour pressure of the compound.
In practice, ho~ever, when a glass substrate is used, the upper lim.it of To is generally determined by the softening point of the substrate glass. It should be noted that the lattice direction of the growing surface in A~E growth most efficiently minimizes the vapour pressure of the compound. This has been established e.g. in connection with CdSe growth, which has been carried out at To ~ 500C without any detectable back evaporation of the compound.
It is obvious that A~E growth is obtainable with several types of growing equiprnent. The essential features are the sovrce and substrate ternperatures, and step~ise interactions bet~een the substrate and the elernent vapours of the compound in rotation. ~specially ~he II-VI compound group offers great freedoln in ecluipment design, due to the high vapour pressure i066174 ~ .
oX II ~nd ~TI elerne~ts. Two principal arrangements dif-ferent fxom that de.i;cribed in ~'ig. 5 are presented in Figs. 6 and 7.
In AIE growth the interaction with a component vapou~
may be o~tained by using a gaseous compound of the element ~'nich decomposcs on the reacting surface, in analogy with the practice of chemical vapour deposition. This kind o~ reaction ma~ be accomplished e.g. with H2S, instead of S2. ~he corresponding ~urface reactions in the case of ZnS growth are X2S(g) + Zn(s) --~ ZnS(s) + H2(g) in the case of H2S, corresponding to the reaction - S2(g) + 2 Zn(s) > ZnS(s) for pure S2 gas. According to the AIæ principle the r~actions-are only possible as long as free Zn(s) surface atoms are available, ~he A~E procedure can be performed with the aid of sputter-type deposition of the component elements. In this .
case there is an inert gas or plasma present in the reaction ~ steps.
~ hen applying equation (1) to surfaces which are not per~ectly covered with the atoms causing surface reaction with the gas atoms in question~ the equation shall only be applied to the active portion of the surface. It an AB compound is grown using partial surface coverage in each or one of the process steps, the equation (1) may be modified to read ~A ~ AB
* N tab PA - PB ~ e s (4) for A-atom reaction steps and UB BA
~s tBA
P~ PA - e - (5) for B atom reaction steps, where PB and PA represent the relative coverages of B and ~ atoms on the surface before the A and B
reaction steps, respectively.
I~r ~` ~066'17~
The p~rtial coverage oi one component clement is of special irnp~ ce w]lein 7rowing cornpound films with low va~our pressure elemen-i~s o with compounds which contain different amounts of the c~mponent elements. An important exarnple of the first-mentioned is the growth of III-V compounds on a substrate which cannot be heated temperature To h:igh enough to ensure perfect back evaporation of the group III elernents. In such a case the surface reaction between group V surface atoins and and group III gaseous atoms is limited -to cause only partial coverage of group III atoms to ensure the absence of super-numerary group III atoms on the surface. ~he group V gas reaction with the surface partially covered with g~oup III
atoms can be made perfect enough to ensure the oriented nuclea-tion-free A~E growth of the compound.
Another ~mportant case in which partial surface reac-tion æteps have to be used is the growth of dioxides of elements which also have stable or relatively stable monoxi2es. The growth of tin dioxide b~ A~E technique is an illustrative example. In order to form SnO2, instead of SnO, the interaction of Sn vapour with the O surface is restricted to cause Sn coverage of a fe~ per cent only. ~he 2 interaction, effected by me~ls f 2 plasma, ensures the maximuTn nurnber of oxygen atoms to be bonded with Sn atoms, thus causing the dioxide -growth. A strong indication for use of A~E growth in such instances, too, has emerged from the observation t'nat the SnO2 layer on a glass plate shows electrical conductivity in the plane of the surface starting frorn 10 A SnO2 thic]~ness. The conductlvity shows no tumlelling effects, which is proof that the film has a continuous . crystal structure. Such films are physically extremely firm and che.nically resistant, which is in fact true for all compound filrns made by A~E techni~ues, no mattcr w}lether witn perIcc-t or partial covera~e of -the reactin~ surfacc in the individual 7~
~eaction st~p~
E~
_a~ le 1 Al,E growth for ZnS has been carried out with an equipment of ~i~s. 1 and 2 with following values of system parameter3:
- Speed of rotati.on 2 r/s - substrate material: Corning Glass 7059 - substrate temperature 320C, -the total bombardme-nt of Zn-atoms during one interaction bet~/een the surface and .
Zn vapou.r about 5 x 1015 atoms/cm2, which was measured with a quar~.crystal rate monitor, corresponding to an effective Zn vapour pressure of about 10 3 torr and equiLibri~m ~: .
temperature of about 290C for the Zn source - equilibrium temperature of the S source 100C, corresponding to a vapour pressure.of about 10 2 torr and total bombardment of S2 molecules of about 5 x 1016 molecules/cm2.
~ or a ten minutes pr~cess the film thickness was about 0.27 ~m5 for processes of 20 and ~0 minutes the thich~nesses were about 0.54 ~m and 0.80 ~ respectively.
The film structure was examined by etching techniques.
Example 2 -- A~ growth of SnO2 layers on Corning Glass 7059 substrates has been carried out using thc equipment of ~igs. 1 and.2 as follows:
- The substrate temperature ~00C
- The total amount of Sn atoms during one interaction with Sn source about 0.6 1014 atoms/cm2 .. - oxygen source is of plasma type with 10-100 mTorr total pressu.re and 40mA plas.ma cur~ent. The total bombardment of . 30 02 ions being ~ 7 1014 ions/cm2 during the interaction with the plasma source Ib " ` ~ 7~
- with speed rot:ation 1 r/s this proccss ~ives a ~rowth o~ S;~02 ~, O
film to 6~)0A in 25 minutes giVillg 0. 4.~ average growth rate during each ro1ation ~xam~le 3 A~E growth of GaP-layers on CGrning Glass 7059 substrates has been carried out using the equipment of ~i~s.
~ and 2 as follows:
- the ~ubstrate tem-perature~V300C
- the total a~nount of Ga atoms during the interacti.on with ~a source~ 1015 atoms/cm2 - the total amount of P molecules (most probably P4) bornbarding the surface during the interaction with Phosphorus oven is about 5 ' 1015 atoms/cm~
- a 0.25 p film was gro~m with these parar/1eters of substrate and sources in 25 minutes with rotation speed 1 r/s. Average growth rate was 1.7A during each cycle.
Exan~le 4 A~E grow-th of ZnS has been carried out using the equip-men-t of Fig. 7 with follo~ing system parameters: -- substrate c.g. 7059 - substrate temperature~470C
- temperature of Zn-sourcer~ 390C
- temperature of S-source~120C
- interactlon time of the Zn-source 6 sec-onds - escape time of the Zn-vapour 2 seconds - interaction time of the S-source 2 seconds - escape time of the S2-vapour 6 seconds - ~he growth occured at maximum speed within the accuracy of thiclmess measu~ent thus corresponding full coverage at each reaction step. With a 140 min process the film thickness was O,1 2 ~lm.
~x~perl~ncnts wi-th the self--balanclng ~E growth have .
~i7 . ........... ~k -f ~ 7 4 establis.~d ~ f~ct, th~t the trlo~oretical ro~rth speed ca~not be exeeded bu-t apnro~ched ..sympcoticall~J with increased time (or pres~ure) of interact;ion at each reacti.on step.
Selective e-tcning of the ZnS films made by A~E techniques has been performed Wi ch the ai~ o.t a e-tchan-t con tainin~ 60 parts H3P04, 5 parts I~03 and one part H~ at room temperature. ~he etching speed was from 10 ~m/s to 150 ~/s in the direction of the surface for 0.1 to 0.'7 ~m thick %nS films whilst no etchin~
effec t could be ~etected in the direction perpendicularly to the surface plane. ~ching of A~-SnO2 fi.lms has been possible only by electrochemical methods~
1~
Claims (3)
1. A method of growing compound thin films of single atomic layers by sequential surface reaction steps between the single elements of said compound and a body surface, which comprises subjecting in each reaction step said body surface to interaction with atoms of a single element in vapour phase at a partial pressure sufficiently high and over a period of time sufficiently long to cause collisions on said surface of said single element atoms in excess of the number of atoms in one single atomic layer of said surface, and maintaining said surface at a temperature sufficiently high for said surface reaction to occur and too high for the reacting vapour to condense itself on said surface.
2. A method as defined in claim 1, wherein said reacting vapour is a compound of said single element.
3. A method as defined in claim 1, wherein said reacting vapour is said single element itself.
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1975
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- 1975-11-24 IN IN2234/CAL/75A patent/IN143912B/en unknown
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- 1975-11-25 US US05/635,233 patent/US4058430A/en not_active Expired - Lifetime
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- 1975-11-28 FR FR7536480A patent/FR2292517A1/en active Granted
- 1975-11-28 DK DK539875A patent/DK152060C/en not_active IP Right Cessation
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1985
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